CN104342625A - Method for manufacturing black borosilicate glass by vacuum coating - Google Patents
Method for manufacturing black borosilicate glass by vacuum coating Download PDFInfo
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- CN104342625A CN104342625A CN201410109924.5A CN201410109924A CN104342625A CN 104342625 A CN104342625 A CN 104342625A CN 201410109924 A CN201410109924 A CN 201410109924A CN 104342625 A CN104342625 A CN 104342625A
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- Prior art keywords
- borosilicate glass
- coated
- vacuum chamber
- glass
- coating
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Classifications
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/56—Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks
- C23C14/568—Transferring the substrates through a series of coating stations
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/0021—Reactive sputtering or evaporation
- C23C14/0036—Reactive sputtering
Abstract
The invention discloses a method for manufacturing black borosilicate glass by adopting the multi-cavity magnetron sputtering technology. According to the method, before being coated, the glass is cleaned up; then, the glass is conveyed to a pre-vacuum chamber of a vacuum coating device through a conveying device and enters a sputtering coating chamber matched with a large type titanium aluminum magnetic control target later on; nitrogen argon mixed gas is led into the coating chamber; voltage is exerted on the magnetic control target, and glow discharge is generated; a black TiAlN function thin film is deposited on the surface of the borosilicate glass in a reactive sputtering mode; through coated annealing treatment, internal stress of the thin film is further reduced, and the film-based interface combination force is improved. The method for manufacturing the black borosilicate glass by vacuum coating can adjust changes of blackness and transparency of the thin film through changing of components and discharging characteristics; the manufacturing method is high in maneuverability and suitable for industrial batch production and processing.
Description
Technical field
The present invention relates to a kind of preparation method and Preparation equipment of glass, particularly relate to method and Preparation equipment that black borosilicate glass are prepared in a kind of vacuum plating.
Background technology
Devitrified glass is a kind of material having excellent light, heat, electricity, mechanical property and enrich color.Devitrified glass is widely used in the fields such as building, new forms of energy, electronic information and high-grade household electrical appliances as structured material, photoelectric functional material and finishing material.Although devitrified glass is widely used because of its characteristic, but the production comprehensive energy consumption height preparing devitrified glass is Problems existing always, and therefore, industry all a kind ofly can substitute devitrified glass and produce the low glass material of comprehensive power consumption striving to find.
Borosilicate glass are a kind of materials with low thermal expansion, high temperature resistant, the series of advantages such as high transmission rate and high chemical stability, but borosilicate glass are but difficult to the color prepared as devitrified glass so enriches.Therefore, constructing abundant color on extraordinary borosilicate glass surface through vacuum plating process is the effective way that part replaces devitrified glass application, and it can significantly reduce costs, application prospect and market huge.
Coated glass is a kind of secondary processing product of Glass Surface Modification.By various physics or chemical process, certain element or compound are attached to glass surface and give glass surface property, make it to become the New function glass material having and enrich color.
Magnetron sputtering plating at home and abroad developed in recent years and a kind of new and high technology be applied, this technology because of its environmental protection, can plate that material is wide, quality of forming film is high, Application Areas extended capability is strong and becomes a kind of glass coating preparation method of great potential, and also for the extraordinary borosilicate glass film of exploitation provides a kind of effective means.
At present, the product of coated glass mainly comprises two aspects: be photo-thermal controlling diaphragm on the one hand; The function film that imparting film surface has property on the other hand.Wherein, the production technology process of photo-thermal controlling diaphragm is day by day ripe, and range of product and function day by day increase, range of application expanding day.Meanwhile, there is the development also first meeting clue of the function film of property, and just becoming main trend and the growth point of coated glass development.But adopting vacuum coating technology to carry out surface deposition black PVD film to the borosilicate glass with special purpose does not also have special proven technique at home and abroad.
Summary of the invention
The invention provides a kind of method adopting multi-chamber continous way magnetron sputtering technique to prepare black borosilicate glass, it is characterized in that, described method specifically comprises the following steps:
(1) borosilicate glass to be coated are served travelling belt, by travelling belt described borosilicate glass to be coated are delivered to the glass cleaning line in filming equipment, utilize glass cleaning line to clean borosilicate glass to be coated, then air-dry;
(2) borosilicate glass to be coated after air-dry enter the first pre-vacuum chamber in filming equipment by travelling belt, the first pre-vacuum chamber forvacuum;
(3) borosilicate glass to be coated are from the first pre-vacuum chamber by least one coating chamber travelling belt feeding filming equipment, and the vacuum tightness that at least one coating chamber described has been evacuated in vacuum chamber is less than or equal to 5 × 10
-3pa; The first filming indoor are wherein filled with argon nitrogen mixture gas, argon and oxide gas are high-purity gas, the ratio of nitrogen and argon gas is 2:1, gas magnetic controlling target applies voltage and produces glow discharge, argon nitrogen mixture gas carries out reactive sputter-deposition metal nitride film, and target current regulation and control are between 20A-40A;
Described borosilicate glass to be coated are at the uniform velocity advanced in coating chamber, and namely borosilicate glass to be coated are at least introduced into the first filming room from the first pre-vacuum chamber, metal refining nitride film;
(4) borosilicate glass after plated film, by the second pre-vacuum chamber, leave filming equipment from the second pre-vacuum chamber;
(5) borosilicate glass after shifting out from filming equipment carry out follow-up low-temperature annealing process, reduce the internal stress of film further and improve film base interface binding power.
Alternately, described filming equipment comprises more than 2 or 3 coating chambers, and borosilicate glass to be coated need coating film treatment in more than 2 or 3 coating chambers.
Preferably, the annealing temperature in described step (5) controls at 150-300 DEG C, and annealing time is 1-2 hour.
Preferably, the annealing temperature in described step (5) controls at 200 °.
Preferably, the target current regulation and control in described step (3) are at 30A.
Preferably, described the first filming indoor employing 2-6 inlet mouth input gas, to ensure the homogeneity of reaction and sputter gas.
Preferably, in described step (3), target power supply used is direct supply, the pulse power or intermediate frequency power supply.
Preferably, the target adopted in the first filming room in described step (3) is TiAl alloy target or Ti metal targets and Al metal targets.
Preferably, described target is planar targets or column target.
In the method, every sheet glass to be coated from clean to shift out consumed time controling at 4-10 minute from filming equipment.
Present invention also offers a kind of multi-chamber continous way magnetic-controlled sputtering coating equipment, it is characterized in that, described equipment comprises glass cleaning line adjacent successively and at least three vacuum chambers, also be included in glass cleaning line and at least three vacuum chambers that cycle rotation is to transport the travelling belt of glass, described at least three vacuum chambers comprise the first pre-vacuum chamber, at least one coating chamber, the second pre-vacuum chamber; Described first pre-vacuum chamber forvacuum, borosilicate glass to be coated are from the first pre-vacuum chamber by least one the continuous coating room travelling belt feeding filming equipment, and the vacuum tightness that at least one coating chamber described can be evacuated in vacuum chamber is less than or equal to 5 × 10
-3pa; The first filming indoor are wherein filled with argon nitrogen mixture gas, argon and oxide gas are high-purity gas, and the ratio of nitrogen and argon gas is 2:1, and magnetic controlling target applies voltage and produces glow discharge, argon nitrogen mixture gas carries out reactive sputter-deposition metal nitride film, and target current regulation and control are between 20A-40A; Described borosilicate glass to be coated at the uniform velocity can be advanced in coating chamber, and namely borosilicate glass to be coated are at least introduced into the first filming room from the first pre-vacuum chamber, metal refining nitride film; Borosilicate glass after plated film, by the second pre-vacuum chamber, leave filming equipment from the second pre-vacuum chamber.
By the black borosilicate glass product that the present invention adopts magnetron sputtering technique to prepare at borosilicate glass surface deposition, multiple special dimension can be used for by Some substitute devitrified glass.The method of black borosilicate glass is prepared in vacuum plating provided by the invention, and by the change of composition and discharge characteristic, the change of adjustment film blackness and transparence, preparation method is workable, is applicable to industrialized mass production processing.
Accompanying drawing explanation
Fig. 1 is multi-chamber continous way magnetic-controlled sputtering coating equipment structural representation.
Embodiment
Hereafter will describe the preferred embodiments of the present invention in detail, to the present invention, how utilisation technology means solve technical problem whereby, and the implementation procedure reaching technique effect can fully understand and implement according to this.
Embodiment 1
The invention provides a kind of multi-chamber continous way magnetic-controlled sputtering coating equipment, described filming equipment structure as shown in Figure 1, comprises travelling belt 1 and three vacuum chambers, and three vacuum chambers comprise the first pre-vacuum chamber 3, the first filming room 4 and the second pre-vacuum chamber 5.Described first pre-vacuum chamber 3 is positioned at before the first filming room 4, and the second pre-vacuum chamber 6 is positioned at after the first filming room 4, travelling belt in the first pre-vacuum chamber, the first filming room, the second pre-vacuum chamber cycle rotation to transport borosilicate glass to be coated.In addition, also provide glass cleaning line 2, for carrying out cleaning and air-dry to borosilicate glass to be coated, described glass cleaning line 2 is connected with the first pre-vacuum chamber 3 and is integrated, and travelling belt is simultaneously through glass cleaning line 2.Glass after cleaning directly enters the first pre-vacuum chamber 3 after air-dry, first pre-vacuum chamber 3 forvacuum, borosilicate glass to be coated send into the first filming room 4 from the first pre-vacuum chamber 3 by travelling belt, and the vacuum tightness that coating chamber 4 can be evacuated in vacuum chamber is less than or equal to 5 × 10
-3pa; Be filled with argon nitrogen mixture gas in the first filming room 4 wherein, magnetic controlling target applies voltage and produces glow discharge, and argon nitrogen mixture gas carries out reactive sputter-deposition metal nitride film, and target current regulation and control are between 20A-40A;
Described borosilicate glass to be coated at the uniform velocity can be advanced in coating chamber, and speed can be 0.5m/min, and the time that described every sheet glass to be coated passes in and out the travelling belt of continuous sputtering coating equipment can control at 5-10min.
Preferably, the argon that the first filming room 4 is used and oxide gas are high-purity gas, and the ratio of nitrogen and argon gas is 2:1.
Preferably, 2-6 inlet mouth input gas is adopted in the first filming room 4, to ensure the homogeneity of reaction and sputter gas.
The invention provides a kind of method adopting multi-chamber continous way magnetron sputtering technique to prepare black borosilicate glass, described method specifically comprises the following steps:
(1) cleaning and air-dry is carried out to borosilicate glass to be coated;
Particularly, utilize glass cleaning line to clean borosilicate glass to be coated, described glass cleaning line is connected with the first pre-vacuum chamber and is integrated, and the glass after cleaning directly enters the first pre-vacuum chamber after air-dry.
(2) the first pre-vacuum chamber in continuous coating device delivered to by described borosilicate glass to be coated by travelling belt, the first pre-vacuum chamber forvacuum;
(3) borosilicate glass to be coated send into coating chamber by travelling belt, and at the uniform velocity advance in coating chamber, namely treat that glass plating enters the first filming room from the first pre-vacuum chamber, metal refining nitride film.
The vacuum tightness that the first filming room has been evacuated in vacuum chamber is less than or equal to 5 × 10
-3pa;
Particularly, vacuum tightness reaches 5 × 10
-3the Pa time used is 30-60min.
The first filming indoor are filled with argon nitrogen mixture gas, and magnetic controlling target applies voltage and produces glow discharge, and argon nitrogen mixture gas carries out reactive sputter-deposition metal nitride film, and target current regulates and controls between 20A-40A, preferred 30A;
Particularly, the argon that the first filming room is used and oxide gas are high-purity gas, and the ratio of nitrogen and argon gas is 2:1, and described the first filming indoor employing 2-6 inlet mouth input gas, to ensure the homogeneity of reaction and sputter gas.
Preferably, target is TiAl alloy target or Ti and Al metal targets, and the metal nitride film of deposition is TiAlN film, and target is planar targets or column target.
The target power supply adopted in described the first filming room is particularly direct supply, the pulse power or intermediate frequency power supply.
Preferably, every sheet glass to be coated is at the uniform velocity advanced in continuous sputter coating indoor, and speed can be 0.5m/min, and the time that described every sheet glass to be coated passes in and out the travelling belt of continuous sputtering coating equipment can control at 4-10min.
(4) borosilicate glass after plated film, by the second pre-vacuum chamber, leave filming equipment from the second pre-vacuum chamber;
(5) borosilicate glass after plated film carry out follow-up low-temperature annealing process, and annealing temperature controls at 150-300 DEG C, and annealing time is 1-2 hour.Anneal after plated film reduces the internal stress of film further and improves film base interface binding power.
Particularly, the glass after plated film need carry out anneal as early as possible, starts subsequent anneal process in 30 minutes preferably after plated film terminates, and does not the longlyest exceed 90 minutes.Annealing temperature preferably 200 °.
Embodiment 2
Embodiment 2 provides a kind of multi-chamber continous way magnetic-controlled sputtering coating equipment, and described filming equipment, except all structures comprising embodiment 1, also comprises the second coating chamber, and the second coating chamber is between the first filming room 4 and the second pre-vacuum chamber 5.
Correspondingly, embodiment 2 prepare in the method for black borosilicate glass, borosilicate glass to be coated, after the coating film treatment in the first filming room 4, enter the second coating chamber and carry out further coating film treatment, and then enter the second pre-vacuum chamber 5.In example 2, the first filming room metal refining nitride film, same metal refining nitride film in the second coating chamber.
Be filled with argon nitrogen mixture gas in second coating chamber, magnetic controlling target applies voltage and produces glow discharge, and argon nitrogen mixture gas carries out reactive sputter-deposition metal nitride film, and target current regulates and controls between 20A-40A, preferred 30A; Particularly, the second coating chamber is used for metal refining nitride film, and argon used and oxide gas are high-purity gas, and the ratio of nitrogen and argon gas is 2:1, adopts 2-6 inlet mouth input gas, to ensure the homogeneity of reaction and sputter gas in described second coating chamber.
Particularly, target used in described second coating chamber is TiAl alloy target or Ti and Al metallic target, and described target is planar targets or column target;
Particularly, in described second coating chamber, target power supply used is direct supply, the pulse power or intermediate frequency power supply.
Embodiment 3
Embodiment 3 provides a kind of multi-chamber continous way magnetic-controlled sputtering coating equipment, described continuous sputtering coating equipment is except all structures comprising embodiment 1, also comprise at least the second coating chamber and the 3rd coating chamber, at least the second coating chamber and the 3rd coating chamber are between the first filming room 4 and the second pre-vacuum chamber 5.
Correspondingly, embodiment 3 prepare in the method for black borosilicate glass, borosilicate glass to be coated, after the coating film treatment in the first filming room 4, enter at least the second coating chamber and the 3rd coating chamber carries out further coating film treatment, and then enter the second pre-vacuum chamber 5.In embodiment 3, each coating chamber is metal refining nitride film respectively, such as TiAlN film.
The foregoing is only preferred embodiment of the present invention, be not limited to the present invention, all any amendments, equivalent replacement and improvement etc. made within the present invention's spirit and principle, are all contained within protection scope of the present invention.
Claims (10)
1. adopt multi-chamber continous way magnetron sputtering technique to prepare a method for black borosilicate glass, it is characterized in that, described method specifically comprises the following steps:
(1) borosilicate glass to be coated are served travelling belt, by travelling belt described borosilicate glass to be coated are delivered to the glass cleaning line in filming equipment, utilize glass cleaning line to clean borosilicate glass to be coated, then air-dry;
(2) borosilicate glass to be coated after air-dry enter the first pre-vacuum chamber in filming equipment by travelling belt, the first pre-vacuum chamber forvacuum;
(3) borosilicate glass to be coated are from the first pre-vacuum chamber by least one coating chamber travelling belt feeding filming equipment, and the vacuum tightness that at least one coating chamber described has been evacuated in vacuum chamber is less than or equal to 5 × 10
-3pa; The first filming indoor are wherein filled with argon nitrogen mixture gas, argon and oxide gas are high-purity gas, and the ratio of nitrogen and argon gas is 2:1, and magnetic controlling target applies voltage and produces glow discharge, argon nitrogen mixture gas carries out reactive sputter-deposition metal nitride film, and target current regulation and control are between 20A-40A;
Described borosilicate glass to be coated are at the uniform velocity advanced in coating chamber, and namely borosilicate glass to be coated are at least introduced into the first filming room from the first pre-vacuum chamber, metal refining nitride film;
(4) borosilicate glass after plated film, by the second pre-vacuum chamber, leave filming equipment from the second pre-vacuum chamber;
(5) borosilicate glass after shifting out from filming equipment carry out follow-up low-temperature annealing process, reduce the internal stress of film further and improve film base interface binding power.
2. method according to claim 1, described filming equipment comprises more than 2 or 3 coating chambers, and borosilicate glass to be coated need coating film treatment in more than 2 or 3 coating chambers.
3. method according to claim 1 and 2, the annealing temperature in described step (5) controls at 150-300 DEG C, and annealing time is 1-2 hour.
4. the method according to any one of claim 1-3, the annealing temperature in described step (5) controls at 200 °.
5. the method according to any one of claim 1-4, target power supply used in described step (3) is direct supply, the pulse power or intermediate frequency power supply, and target current regulation and control are at 30A.
6. the method according to any one of claim 1-5, described the first filming indoor employing 2-6 inlet mouth input gas, to ensure the homogeneity of reaction and sputter gas.
7. the method according to any one of claim 1-6, the target adopted in the first filming room in described step (3) is TiAl alloy target or Ti metal targets and Al metal targets, and the metal nitride film of deposition is TiAlN film.
8. method according to claim 7, described target is planar targets or column target.
9. the method according to any one of claim 1-8, every sheet glass to be coated from clean to shift out consumed time controling at 4-10 minute from filming equipment.
10. a multi-chamber continous way magnetic-controlled sputtering coating equipment, it is characterized in that, described equipment comprises glass cleaning line adjacent successively and at least three vacuum chambers, also be included in glass cleaning line and at least three vacuum chambers that cycle rotation is to transport the travelling belt of glass, described at least three vacuum chambers comprise the first pre-vacuum chamber, at least one coating chamber and the second pre-vacuum chamber; Described first pre-vacuum chamber forvacuum, borosilicate glass to be coated are from the first pre-vacuum chamber by least one the continuous coating room travelling belt feeding filming equipment, and the vacuum tightness that at least one coating chamber described can be evacuated in vacuum chamber is less than or equal to 5 × 10
-3pa; The first filming indoor are wherein filled with argon nitrogen mixture gas, argon and oxide gas are high-purity gas, and the ratio of nitrogen and argon gas is 2:1, and magnetic controlling target applies voltage and produces glow discharge, argon nitrogen mixture gas carries out reactive sputter-deposition metal nitride film, and target current regulation and control are between 20A-40A; Described borosilicate glass to be coated at the uniform velocity can be advanced in coating chamber, and namely borosilicate glass to be coated are at least introduced into the first filming room from the first pre-vacuum chamber, metal refining nitride film; Borosilicate glass after plated film, by the second pre-vacuum chamber, leave filming equipment from the second pre-vacuum chamber.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410109924.5A CN104342625A (en) | 2014-03-21 | 2014-03-21 | Method for manufacturing black borosilicate glass by vacuum coating |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410109924.5A CN104342625A (en) | 2014-03-21 | 2014-03-21 | Method for manufacturing black borosilicate glass by vacuum coating |
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| Publication Number | Publication Date |
|---|---|
| CN104342625A true CN104342625A (en) | 2015-02-11 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410109924.5A Pending CN104342625A (en) | 2014-03-21 | 2014-03-21 | Method for manufacturing black borosilicate glass by vacuum coating |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020034967A1 (en) * | 2018-08-13 | 2020-02-20 | 中兴通讯股份有限公司 | Vacuum coating apparatus and method, and preparation method of film layer inside filter cavity |
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| CN1413933A (en) * | 2002-09-06 | 2003-04-30 | 鲍冠中 | Magnetic control sputtering hot-bending coated glass and its production method and device |
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| CN103896497A (en) * | 2012-12-31 | 2014-07-02 | 中国南玻集团股份有限公司 | Single silver thermochromism glass and preparation method thereof |
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2014
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| CN1413933A (en) * | 2002-09-06 | 2003-04-30 | 鲍冠中 | Magnetic control sputtering hot-bending coated glass and its production method and device |
| CN102181839A (en) * | 2011-06-03 | 2011-09-14 | 浙江大学 | Same end entrance-exit type continuous sputtering film plating device |
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| WO2020034967A1 (en) * | 2018-08-13 | 2020-02-20 | 中兴通讯股份有限公司 | Vacuum coating apparatus and method, and preparation method of film layer inside filter cavity |
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Application publication date: 20150211 |
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